CN114291879A - Preparation method of aluminum silicate - Google Patents

Preparation method of aluminum silicate Download PDF

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CN114291879A
CN114291879A CN202111396047.0A CN202111396047A CN114291879A CN 114291879 A CN114291879 A CN 114291879A CN 202111396047 A CN202111396047 A CN 202111396047A CN 114291879 A CN114291879 A CN 114291879A
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silicon
reaction
glucose
containing alkaline
slag
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CN114291879B (en
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伍珍秀
蒋霖
伍金树
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Pangang Group Vanadium Titanium & Resources Co ltd
Pangang Group Research Institute Co Ltd
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Pangang Group Research Institute Co Ltd
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Abstract

The invention relates to the field of chemical industry and discloses a preparation method of aluminum silicate. The method comprises the following steps: (1) adding aluminum sulfate into the silicon-containing alkaline vanadium liquid, reacting under stirring, and then filtering and washing to obtain precipitated slag; (2) adding the precipitation slag obtained in the step (1) into water for pulping, then adding glucose for reaction, then adding ethanol for reaction, and then filtering, washing and drying; wherein the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium liquid is 1: 2.8-3. By using the method disclosed by the invention to treat the sodium vanadate solution obtained after water leaching in the vanadium slag sodium salt roasting-water leaching process, a high-purity aluminum silicate product can be obtained on the premise of ensuring high-efficiency removal of silicon impurities, the discharge of waste is reduced, and resource utilization is realized. The obtained high-purity aluminum silicate product can be directly used as a raw material for producing pigments and coatings.

Description

Preparation method of aluminum silicate
Technical Field
The invention relates to the field of chemical industry, in particular to a preparation method of aluminum silicate.
Background
The sodium salt roasting-water leaching vanadium process of vanadium slag mainly adopts sodium salt as roasting additive, roasting under the condition of high temperature and aerobic condition to produce sodium vanadate dissolved in water, obtaining sodium vanadate solution after water leaching, further precipitating vanadium to obtain vanadium product, but the vanadium slag contains a large amount of silicon, and forms sodium silicate with sodium, and the sodium silicate and sodium silicate also enter the solution together, if the sodium silicate is not removed in the vanadium solution, the quality of precipitated vanadium and vanadium product can be influenced.
For example, the best silicon removal effect by magnesium sulfate is reported in the research on silicon removal by an alkaline vanadium liquid precipitation method, silicon removal is carried out by a flocculating agent in the research on silicon removal test by vanadium-containing alkaline immersion liquid, and phosphorus removal by adding calcium oxide is firstly studied in the research on deep impurity removal process by salt-free roasting leachate, and the silicon removal agent is selected from aluminum hydroxide, so that impurity elements meet the national standard requirements. At present, a large number of documents and patent reports are all limited to simply removing silicon and phosphorus, and the obtained impurity-removed slag needs secondary vanadium extraction or is directly stacked with residue to be used as waste, so that the waste of resources is caused.
Disclosure of Invention
The invention aims to solve the problems that in the prior art, the impurity-removed slag obtained by silicon removal is stored as waste to cause resource waste and environmental pollution, the purity of aluminum silicate obtained by silicon removal is not high, and the like, and provides a preparation method of aluminum silicate.
In order to achieve the above object, the present invention provides a method for preparing aluminum silicate, comprising the steps of:
(1) adding aluminum sulfate into the silicon-containing alkaline vanadium liquid, reacting under stirring, and then filtering and washing to obtain precipitated slag;
(2) adding the precipitation slag obtained in the step (1) into water for pulping, then adding glucose for reaction, then adding ethanol for reaction, and then filtering, washing and drying;
wherein the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium liquid is 1: 2-3.
Preferably, in the step (1), the concentration of silicon in the silicon-containing alkaline vanadium solution is 0.6-3g/L, and the pH value of the silicon-containing alkaline vanadium solution is 9.5-10.5.
Preferably, in the step (1), the reaction temperature is 95-99 ℃ and the reaction time is 30-60 min.
Preferably, the specific process of step (2) comprises: adding the precipitation slag obtained in the step (1) into water, pulping at 95-99 ℃, adding glucose at 95-99 ℃ for heat preservation reaction, cooling to 45-60 ℃, adding ethanol for heat preservation reaction, and then filtering, washing and drying.
Preferably, in the step (2), the solid-to-liquid ratio of the precipitation slag to the water is 1g:1.5-2.5 mL.
Preferably, in the step (2), the weight ratio of the glucose to the precipitation slag is 0.3-0.5: 100.
Preferably, in the step (2), the ethanol is added in an amount of 0.05 to 0.3 vol% based on the volume of the solution obtained by the reaction with glucose.
Preferably, in the step (2), the reaction time of the incubation reaction with the added glucose is 80-180 min.
Preferably, in the step (2), ethanol is added for reaction under heat preservation for 30-60 min.
Preferably, in the step (2), the beating time is 30-45 min.
By using the method disclosed by the invention to treat the sodium vanadate solution obtained after water leaching in the vanadium slag sodium salt roasting-water leaching process, a high-purity aluminum silicate product can be obtained on the premise of ensuring high-efficiency removal of silicon impurities, the discharge of waste is reduced, and resource utilization is realized. The obtained high-purity aluminum silicate product can be directly used as a raw material for producing pigments and coatings.
Detailed Description
The following describes in detail specific embodiments of the present invention. It should be understood that the detailed description and specific examples, while indicating the present invention, are given by way of illustration and explanation only, not limitation.
The endpoints of the ranges and any values disclosed herein are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values. For ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
The invention provides a preparation method of aluminum silicate, which comprises the following steps:
(1) adding aluminum sulfate into the silicon-containing alkaline vanadium liquid, reacting under stirring, and then filtering and washing to obtain precipitated slag;
(2) adding the precipitation slag obtained in the step (1) into water for pulping, then adding glucose for reaction, then adding ethanol for reaction, and then filtering, washing and drying;
wherein the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium liquid is 1: 2-3.
In the invention, in the step (1), the silicon-containing alkaline vanadium solution may be a sodium vanadate solution obtained after water leaching in a vanadium slag sodium salt roasting-water vanadium leaching process.
In a preferred embodiment, in the step (1), the concentration of silicon in the silicon-containing alkaline vanadium solution is 0.6-3g/L, and the pH value of the silicon-containing alkaline vanadium solution is 9.5-10.5.
Further preferably, the concentration of vanadium in the silicon-containing alkaline vanadium solution is 10-60 g/L.
In a preferred embodiment, in step (1), the reaction temperature is 95 ℃ to 99 ℃ and the reaction time is 30 to 60 min. Specifically, the reaction temperature may be 95 ℃, 95.5 ℃, 96 ℃, 96.5 ℃, 97 ℃, 97.5 ℃, 98 ℃, 98.5 ℃ or 99 ℃.
In a preferred embodiment, the specific process of step (2) comprises: adding the precipitation slag obtained in the step (1) into water, pulping at 95-99 ℃, adding glucose at 95-99 ℃ for heat preservation reaction, cooling to 45-60 ℃, adding ethanol for heat preservation reaction, and then filtering, washing and drying. In particular embodiments, the temperature of the beating may be 95 ℃, 95.5 ℃, 96 ℃, 96.5 ℃, 97 ℃, 97.5 ℃, 98 ℃, 98.5 ℃ or 99 ℃; the temperature of the heat preservation reaction by adding glucose can be 95 ℃, 95.5 ℃, 96 ℃, 96.5 ℃, 97 ℃, 97.5 ℃, 98 ℃, 98.5 ℃ or 99 ℃; the temperature of the heat-preservation reaction by adding ethanol can be 45 ℃, 46 ℃, 47 ℃, 48 ℃, 49 ℃, 50 ℃, 51 ℃, 52 ℃, 53 ℃, 54 ℃, 55 ℃, 56 ℃, 57 ℃, 58 ℃, 59 ℃ or 60 ℃.
In the present invention, the precipitation sludge obtained by washing in the step (1) is directly used in the step (2), and therefore, the weight of the precipitation sludge in the step (2) in the present invention is the wet weight of the precipitation sludge.
In a preferred embodiment, in the step (2), the solid-to-liquid ratio of the precipitation slag to the water is 1g:1.5-2.5 mL. Specifically, the solid-to-liquid ratio of the sludge to water may be 1g:1.5mL, 1g:1.6mL, 1g:1.7mL, 1g:1.8mL, 1g:1.9mL, 1g:2mL, 1g:2.1mL, 1g:2.2mL, 1g:2.3mL, 1g:2.4mL, or 1g:2.5 mL.
In a preferred embodiment, in step (2), the weight ratio of the glucose to the precipitation sludge is 0.3-0.5: 100. Specifically, the weight ratio of the glucose to the precipitation sludge may be 0.3:100, 0.35:100, 0.4:100, 0.45:100, or 0.5: 100.
In a preferred embodiment, in the step (2), the ethanol is added in an amount of 0.05 to 0.3 vol% based on the volume of the solution obtained by the reaction with glucose.
In a preferred embodiment, in step (2), the reaction time for the incubation reaction with the addition of glucose is 80-180 min. Specifically, the time period can be 80min, 90min, 100min, 110min, 120min, 130min, 140min, 150min, 160min, 170min or 180 min.
In a preferred embodiment, in the step (2), ethanol is added for reaction under heat preservation for 30-60 min. Specifically, the time period can be 30min, 35min, 40min, 45min, 50min, 55min or 60 min.
In a preferred embodiment, in step (2), the beating time is 30-45 min. Specifically, the time period can be 30min, 31min, 32min, 33min, 34min, 35min, 36min, 37min, 38min, 39min, 40min, 41min, 42min, 43min, 44min or 45 min.
In a preferred embodiment, in step (2), washing is performed with hot water. Further preferably, the temperature of the hot water is 80-95 ℃.
The present invention will be described in detail below by way of examples, but the scope of the present invention is not limited thereto.
The silicon-containing alkaline vanadium solution used in the following examples and comparative examples is a sodium vanadate solution obtained after water leaching in a vanadium slag sodium salt roasting-water vanadium leaching process.
Example 1
(1) Adding aluminum sulfate into silicon-containing alkaline vanadium liquid (the pH value is 9.5, the Si concentration is 0.6g/L, the vanadium concentration is 10g/L), wherein the molar ratio of the aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:3, stirring and reacting for 30min at 95 ℃, and then filtering and washing to obtain precipitation slag;
(2) adding the precipitation slag obtained in the step (1) into water, pulping for 30min at 95 ℃, keeping the solid-liquid ratio of the wet weight of the precipitation slag to the water at 1g:1.5mL, then adding glucose (the wet weight ratio of the glucose to the precipitation slag is 0.3:100) at 95 ℃, preserving heat, reacting for 80min, naturally cooling to 45 ℃, adding ethanol, preserving heat, reacting for 30min, wherein the adding amount of the ethanol is 0.05 vol% of the volume of the solution obtained by adding the glucose and carrying out the heat preservation reaction, and then filtering, washing with hot water and drying.
Example 2
(1) Adding aluminum sulfate into silicon-containing alkaline vanadium liquid (the pH value is 10, the Si concentration is 1.6g/L, and the vanadium concentration is 20g/L), wherein the molar ratio of the aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:3, stirring and reacting for 45min at 97 ℃, and then filtering and washing to obtain precipitation slag;
(2) adding the precipitation slag obtained in the step (1) into water, pulping for 38min at 96 ℃, keeping the solid-to-liquid ratio of the wet weight of the precipitation slag to the water at 1g:2mL, then adding glucose (the wet weight ratio of the glucose to the precipitation slag is 0.4:100) at 96 ℃, carrying out heat preservation reaction for 140min, naturally cooling to 50 ℃, adding ethanol, carrying out heat preservation reaction for 45min, wherein the adding amount of the ethanol is 0.18 volume percent of the volume of the solution obtained by adding the glucose and carrying out the heat preservation reaction, and then filtering, washing with hot water and drying.
Example 3
(1) Adding aluminum sulfate into silicon-containing alkaline vanadium liquid (the pH value is 10, the Si concentration is 3g/L, and the vanadium concentration is 25g/L), wherein the molar ratio of the aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:3, stirring and reacting for 60min at 98 ℃, and then filtering and washing to obtain precipitation slag;
(2) adding the precipitation slag obtained in the step (1) into water, pulping for 45min at 98 ℃, keeping the solid-liquid ratio of the wet weight of the precipitation slag to the water at 1g:2.5mL, then adding glucose (the wet weight ratio of the glucose to the precipitation slag is 0.5:100) at 98 ℃, carrying out heat preservation reaction for 180min, naturally cooling to 60 ℃, adding ethanol for carrying out heat preservation reaction for 60min, wherein the adding amount of the ethanol is 0.3 vol% of the volume of the solution obtained by adding the glucose for carrying out the heat preservation reaction, and then filtering, washing with hot water and drying.
Example 4
(1) Adding aluminum sulfate into silicon-containing alkaline vanadium liquid (the pH value is 9.5, the Si concentration is 0.6g/L, the vanadium concentration is 30/L), wherein the molar ratio of the aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:2.5, stirring and reacting for 30min at 95 ℃, and then filtering and washing to obtain precipitation slag;
(2) adding the precipitation slag obtained in the step (1) into water, pulping for 30min at 95 ℃, keeping the solid-liquid ratio of the wet weight of the precipitation slag to the water at 1g:1.5mL, then adding glucose (the wet weight ratio of the glucose to the precipitation slag is 0.3:100) at 95 ℃, preserving heat, reacting for 80min, naturally cooling to 45 ℃, adding ethanol, preserving heat, reacting for 30min, wherein the adding amount of the ethanol is 0.05 vol% of the volume of the solution obtained by adding the glucose and carrying out the heat preservation reaction, and then filtering, washing with hot water and drying.
Example 5
(1) Adding aluminum sulfate into silicon-containing alkaline vanadium liquid (the pH value is 10, the Si concentration is 1.6g/L, and the vanadium concentration is 20g/L), wherein the molar ratio of the aluminum sulfate to Si in the silicon-containing alkaline vanadium liquid is 1:2, stirring and reacting for 45min at 97 ℃, and then filtering and washing to obtain precipitation slag;
(2) adding the precipitation slag obtained in the step (1) into water, pulping for 38min at 96 ℃, keeping the solid-to-liquid ratio of the wet weight of the precipitation slag to the water at 1g:2mL, then adding glucose (the wet weight ratio of the glucose to the precipitation slag is 0.4:100) at 96 ℃, carrying out heat preservation reaction for 140min, naturally cooling to 50 ℃, adding ethanol, carrying out heat preservation reaction for 45min, wherein the adding amount of the ethanol is 0.18 volume percent of the volume of the solution obtained by adding the glucose and carrying out the heat preservation reaction, and then filtering, washing with hot water and drying.
Comparative example 1
The process is carried out as in example 1, except that in step (1), the molar ratio of aluminium sulphate to Si in the silicon-containing alkaline vanadium solution is 1: 3.2.
Comparative example 2
The process is carried out as in example 1, except that in step (1), the molar ratio of aluminium sulphate to Si in the silicon-containing alkaline vanadium solution is 1: 1.8.
Test example
1. The Si concentrations of the filtrates obtained in step (1) in the examples and comparative examples were measured, and the results are shown in Table 1.
TABLE 1
Numbering Si concentration g/L in silicon-containing alkaline vanadium liquid The concentration of Si in the filtrate is g/L
Example 1 0.6 0.025
Example 2 1.6 0.038
Example 3 3.0 0.15
Example 4 0.6 0.015
Example 5 1.6 0.018
Comparative example 1 0.6 0.082
Comparative example 2 0.6 0.014
2. The purity of the aluminum silicate obtained in the examples and comparative examples was measured and the results are shown in Table 2.
TABLE 2
Numbering Purity of aluminum silicate/%)
Example 1 99.56
Example 2 99.68
Example 3 99.79
Example 4 99.62
Example 5 99.74
Comparative example 1 99.66
Comparative example 2 94.28
From the results in tables 1 and 2, it can be seen that the method of the present invention can effectively remove silicon as an impurity from the silicon-containing alkaline vanadium solution, and can also obtain a high-purity aluminum silicate product.
The preferred embodiments of the present invention have been described above in detail, but the present invention is not limited thereto. Within the scope of the technical idea of the invention, many simple modifications can be made to the technical solution of the invention, including combinations of various technical features in any other suitable way, and these simple modifications and combinations should also be regarded as the disclosure of the invention, and all fall within the scope of the invention.

Claims (10)

1. A method for preparing aluminum silicate, characterized in that the method comprises the following steps:
(1) adding aluminum sulfate into the silicon-containing alkaline vanadium liquid, reacting under stirring, and then filtering and washing to obtain precipitated slag;
(2) adding the precipitation slag obtained in the step (1) into water for pulping, then adding glucose for reaction, then adding ethanol for reaction, and then filtering, washing and drying;
wherein the molar ratio of the aluminum sulfate to the silicon in the silicon-containing alkaline vanadium liquid is 1: 2-3.
2. The method for preparing aluminum silicate as claimed in claim 1, wherein in the step (1), the concentration of silicon in the silicon-containing alkaline vanadium solution is 0.6-3g/L, and the pH value of the silicon-containing alkaline vanadium solution is 9.5-10.5.
3. A process for the preparation of aluminium silicate according to claim 1 or 2, characterized in that in step (1), the reaction temperature is 95-99 ℃ and the reaction time is 30-60 min.
4. The method for preparing aluminum silicate as claimed in claim 1, wherein the specific process of the step (2) comprises: adding the precipitation slag obtained in the step (1) into water, pulping at 95-99 ℃, adding glucose at 95-99 ℃ for heat preservation reaction, cooling to 45-60 ℃, adding ethanol for heat preservation reaction, and then filtering, washing and drying.
5. The method for preparing aluminum silicate as claimed in claim 1 or 4, wherein in the step (2), the solid-to-liquid ratio of the precipitation slag and water is 1g:1.5-2.5 mL.
6. A process for the preparation of aluminium silicate according to claim 1 or 4, characterized in that in step (2) the weight ratio of said glucose to said precipitated slag is 0.3-0.5: 100.
7. The method for preparing aluminum silicate as claimed in claim 1 or 4, wherein in the step (2), said ethanol is added in an amount of 0.05-0.3 vol% based on the volume of the solution obtained by the reaction with glucose.
8. A process for preparing aluminium silicate according to claim 4, wherein in step (2), the reaction time for the incubation reaction with the addition of glucose is 80-180 min.
9. A process for preparing aluminium silicate according to claim 4 or 8, characterized in that in step (2), the reaction time for the incubation reaction with the addition of ethanol is 30-60 min.
10. A process for the preparation of aluminium silicate according to claim 5, characterized in that in step (2), the pulping time is 30-45 min.
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